CN115231532A - Preparation method and application of lithium bis (fluorosulfonyl) imide - Google Patents
Preparation method and application of lithium bis (fluorosulfonyl) imide Download PDFInfo
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- CN115231532A CN115231532A CN202210940057.4A CN202210940057A CN115231532A CN 115231532 A CN115231532 A CN 115231532A CN 202210940057 A CN202210940057 A CN 202210940057A CN 115231532 A CN115231532 A CN 115231532A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/086—Compounds containing nitrogen and non-metals and optionally metals containing one or more sulfur atoms
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to the field of lithium ion battery electrolyte materials, in particular to a preparation method and application of lithium bis (fluorosulfonyl) imide. The invention provides a preparation method of lithium bis (fluorosulfonyl) imide, which comprises the following steps: mixing the bis-fluorosulfonyl imide and lithium halide, reacting above the melting point of the bis-fluorosulfonyl imide to obtain a crude product of the bis-fluorosulfonyl imide, and purifying the crude product of the bis-fluorosulfonyl imide to obtain the lithium bis-fluorosulfonyl imide. According to the invention, the bifluoro-sulfimide and the lithium halide are mixed and then react above the melting point of the bifluoro-sulfimide lithium, so that the yield of the bifluoro-sulfimide lithium can be greatly improved; meanwhile, no other solvent is added in the mixing reaction, so that the impurity content in the crude product of the lithium bis (fluorosulfonyl) imide is reduced, and the impurity content of the purified lithium bis (fluorosulfonyl) imide is effectively reduced.
Description
Technical Field
The invention relates to the field of lithium ion battery electrolyte materials, in particular to a preparation method and application of lithium bis (fluorosulfonyl) imide.
Background
The lithium bis (fluorosulfonyl) imide is a key high-performance electrolyte material in lithium ion batteries, has high conductivity, hydrolysis resistance and electrochemical stability, has an application prospect of possibly replacing lithium hexafluorophosphate and partially replacing lithium hexafluorophosphate, and has a huge industrial application value.
In the prior art, the preparation method of lithium bis (fluorosulfonyl) imide mainly comprises the following two methods: 1) Preparing crude product lithium bis (fluorosulfonyl) imide by using bis (fluorosulfonyl) imide and lithium carbonate or lithium hydroxide, and purifying to obtain high-purity lithium bis (fluorosulfonyl) imide; 2) Reacting the difluoride sulfimide with lithium halide to obtain crude product of the difluoride sulfimide lithium, and purifying to obtain the difluoride sulfimide lithium with higher purity. However, the above methods are all prepared under the low temperature condition in the presence of a solvent, and the yield is low; and because the reaction is carried out in a solvent, impurities are inevitably introduced, so that the content of the impurities in the obtained lithium bis (fluorosulfonyl) imide is high; and when the reaction raw material is lithium carbonate or lithium hydroxide, water is generated in the reaction process, and other reagents are required to be introduced for water removal treatment, so that the content of impurities in the lithium bis (fluorosulfonyl) imide is further increased.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects that the method for preparing the lithium bis (fluorosulfonyl) imide in the prior art is low in yield and high in impurity content of the obtained lithium bis (fluorosulfonyl) imide, so that the preparation method and the application of the lithium bis (fluorosulfonyl) imide are provided.
The invention provides a preparation method of lithium bis (fluorosulfonyl) imide, which comprises the following steps:
mixing the bis-fluorosulfonyl imide and lithium halide, reacting above the melting point of the bis-fluorosulfonyl imide to obtain a crude product of the bis-fluorosulfonyl imide, and purifying the crude product of the bis-fluorosulfonyl imide to obtain the lithium bis-fluorosulfonyl imide.
The reaction formula of the reaction of the bis-fluorosulfonyl imide and the lithium halide to generate the lithium bis-fluorosulfonyl imide is as follows:
(FSO 2 ) 2 NH+LiX＝(FSO 2 ) 2 NLi+HX
wherein (FSO) 2 ) 2 NH is bis (fluorosulfonyl) imide, liX is lithium halide, (FSO) 2 ) 2 NLi is lithium bis (fluorosulfonyl) imide, and HX is hydrogen halide.
Preferably, the reaction temperature is 124-150 ℃, and preferably, the reaction temperature is 120-130 ℃.
Preferably, the molar ratio of the bis-fluorosulfonyl imide to the lithium halide is (0.1-10): 1;
the reaction time is 5-24h;
the lithium halide is selected from at least one of lithium bromide, lithium iodide, lithium fluoride and lithium chloride, preferably, the lithium halide is selected from at least one of lithium fluoride and lithium chloride.
Preferably, the molar ratio of the bis-fluorosulfonyl imide to the lithium halide is (0.8-1.2): 1.
preferably, no solvent is added during the reaction.
Preferably, the purification step comprises dissolving the crude product of lithium bis (fluorosulfonyl) imide to obtain a lithium bis (fluorosulfonyl) imide solution; and filtering, concentrating, crystallizing, filtering again, washing and drying the lithium bis (fluorosulfonyl) imide solution to obtain the lithium bis (fluorosulfonyl) imide.
Preferably, the solvent for dissolving the crude lithium bis (fluorosulfonyl) imide comprises a first solvent and a second solvent, wherein the first solvent is at least one selected from the group consisting of diethyl ether, propyl ether, tetrahydrofuran, acetonitrile, ethyl acetate, propyl acetate, methyl acetate, dimethyl carbonate, diethyl carbonate, dioxane, acetone, and butanone;
the second solvent is at least one selected from the group consisting of xylene, toluene, benzene, dichlorobenzene, chlorobenzene, difluorobenzene, fluorobenzene, petroleum ether, dichloromethane, dichloroethane, hexane and cyclohexane;
preferably, the first solvent is selected from at least one of diethyl ether, acetonitrile, dimethyl carbonate and diethyl carbonate; the second solvent is at least one selected from the group consisting of dichloromethane, dichloroethane, and toluene.
Preferably, the mass ratio of the first solvent to the second solvent is (9-11): 9.
preferably, the concentration process is vacuum evaporation concentration.
Preferably, the mass ratio of the residue after concentration to the lithium bis (fluorosulfonyl) imide solution is (0.35-0.8): 1;
the concentration temperature is 30-80 ℃.
Preferably, the dissolving temperature is 0-100 ℃, and preferably, the dissolving temperature is 30-60 ℃;
the mass ratio of the crude product of the bis-fluorosulfonyl imide lithium to a solvent for dissolving the crude product of the bis-fluorosulfonyl imide lithium is 1: (1-3).
Preferably, the crystallization and filtration step comprises: and adding a crystallization solvent into the concentrated product, and then filtering to obtain the crystalline lithium bis (fluorosulfonyl) imide.
Preferably, the washing step comprises: washing the crystallized lithium bis (fluorosulfonyl) imide with a washing solvent for 1-3 times; the mass ratio of the washing solvent used in each washing process to the residue after concentration is (0.1-0.8): 1.
Preferably, the crystallization solvent used in the crystallization step is selected from at least one of xylene, toluene, benzene, dichlorobenzene, chlorobenzene, difluorobenzene, fluorobenzene, petroleum ether, dichloromethane, dichloroethane, hexane and cyclohexane;
the washing solvent used in the washing step is at least one selected from the group consisting of xylene, toluene, benzene, dichlorobenzene, chlorobenzene, difluorobenzene, fluorobenzene, petroleum ether, dichloromethane, dichloroethane, hexane and cyclohexane.
Preferably, the drying temperature is 40-80 ℃; the drying time is 3-10h.
Preferably, the method also comprises removing hydrogen halide gas generated in the reaction.
Preferably, the step of removing the hydrogen halide gas generated in the mixing reaction comprises removing by vacuum or blowing nitrogen gas into the reaction system.
The invention also provides application of the bis-fluorosulfonyl imide lithium prepared by the method in preparation of lithium ion battery electrolyte materials.
The technical scheme of the invention has the following advantages:
the invention provides a method for preparing bis (fluorosulfonyl) imide lithium, which comprises the steps of mixing bis (fluorosulfonyl) imide with lithium halide, reacting at a temperature higher than the melting point of the bis (fluorosulfonyl) imide lithium to obtain a crude bis (fluorosulfonyl) imide lithium, and purifying the crude bis (fluorosulfonyl) imide lithium to obtain the bis (fluorosulfonyl) imide lithium. According to the invention, the bifluoro-sulfimide and the lithium halide are mixed and then react above the melting point of the bifluoro-sulfimide lithium, so that the yield of the bifluoro-sulfimide lithium can be greatly improved; meanwhile, no other solvent is added in the mixing reaction, so that the impurity content in the crude product of the lithium bis (fluorosulfonyl) imide is reduced, and the impurity content of the purified lithium bis (fluorosulfonyl) imide is effectively reduced.
According to the preparation method of the lithium bis (fluorosulfonyl) imide provided by the invention, no solvent is required to be added in the reaction process, no water is generated, and no water is required to be removed, so that the reaction process route is short, the required equipment is few, the investment of industrial equipment is greatly reduced, meanwhile, only hydrogen halide is generated as a byproduct, the hydrogen halide can be recycled, and no three wastes are generated.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are conventional reagent products which are commercially available, and manufacturers are not indicated.
Example 1
The embodiment provides a method for preparing lithium bis (fluorosulfonyl) imide, which comprises the following steps:
1) Adding 38.7g of bis (fluorosulfonyl) imide and 6g of lithium fluoride into a reaction bottle, opening a gas absorption device, heating to enable materials in the reaction bottle to react for 5 hours at 130 ℃, blowing the materials in the reaction bottle with nitrogen gas in the reaction process to remove hydrogen fluoride gas generated by the reaction to obtain 38g of crude bis (fluorosulfonyl) imide lithium, wherein the yield of the crude bis (fluorosulfonyl) imide lithium is 95%;
2) Slowly adding 38g of crude bis (fluorosulfonyl) imide lithium obtained in the step 1) into a mixed solvent of 45g of diethyl ether and 45g of dichloroethane for dissolving, obtaining a bis (fluorosulfonyl) imide lithium solution after the crude bis (fluorosulfonyl) imide lithium is completely dissolved at 40 ℃, and cooling the bis (fluorosulfonyl) imide lithium solution to 25 ℃ for filtering; the filtrate was concentrated by vacuum evaporation in a rotary evaporator at 30 ℃ to a residue weight of 65g; slowly adding 50g of dichloroethane into the residue for crystallization, and filtering after crystallization to obtain a filter cake; washing the filter cake 3 times with dichloroethane, wherein the weight of the dichloroethane used in each washing is 50g; and transferring the washed filter cake to a rotary evaporator for drying, and drying at 40 ℃ for 8h to obtain 30g of the lithium bis (fluorosulfonyl) imide. The yield of lithium bis (fluorosulfonyl) imide was 78.9% compared to the weight of crude lithium bis (fluorosulfonyl) imide.
Measuring the content of impurities in the obtained lithium bis (fluorosulfonyl) imide, wherein H 2 O：9ppm；K：2.5ppm；Na：3ppm；Fe<1ppm；Cl<1ppm；SO 4 2 ：9ppm。
Example 2
The embodiment provides a method for preparing lithium bis (fluorosulfonyl) imide, which comprises the following steps:
1) Adding 38.7g of bis (fluorosulfonyl) imide and 6g of lithium fluoride into a reaction bottle, opening a gas absorption device, heating to enable materials in the reaction bottle to react for 5 hours at 130 ℃, blowing the materials in the reaction bottle with nitrogen gas in the reaction process to remove hydrogen fluoride gas generated by the reaction to obtain 38g of crude bis (fluorosulfonyl) imide lithium, wherein the yield of the crude bis (fluorosulfonyl) imide lithium is 95%;
2) Slowly adding 38g of crude bis (fluorosulfonyl) imide lithium obtained in the step 1) into a mixed solvent of 45g of diethyl ether and 45g of toluene for dissolving, obtaining a bis (fluorosulfonyl) imide lithium solution after the crude bis (fluorosulfonyl) imide lithium is completely dissolved at 40 ℃, and cooling the bis (fluorosulfonyl) imide lithium solution to 25 ℃ for filtering; the filtrate was concentrated by vacuum evaporation in a rotary evaporator at 30 ℃ until the weight of the residue became 63g; slowly adding 50g of toluene into the residue for crystallization, and filtering after crystallization to obtain a filter cake; washing the filter cake 3 times by using toluene, wherein the weight of the toluene used for each washing is 50g; the washed filter cake was transferred to a rotary evaporator to be dried and dried at 40 ℃ for 8 hours to obtain 28g of the lithium bis (fluorosulfonyl) imide. The yield of lithium bis (fluorosulfonyl) imide was 73.6% compared to the weight of crude lithium bis (fluorosulfonyl) imide.
Measuring the content of impurities in the obtained lithium bis (fluorosulfonyl) imide, wherein H 2 O：3ppm；K：3ppm；Na：2ppm；Fe<1ppm；Cl<1ppm；SO 4 2 ：12ppm。
Example 3
The embodiment provides a method for preparing lithium bis (fluorosulfonyl) imide, which comprises the following steps:
1) Adding 38.7g of bis (fluorosulfonyl) imide and 6g of lithium fluoride into a reaction bottle, opening a gas absorption device, heating to enable materials in the reaction bottle to react for 5 hours at 130 ℃, blowing the materials in the reaction bottle with nitrogen gas to remove hydrogen fluoride gas generated by the reaction in the reaction process to obtain 38g of crude bis (fluorosulfonyl) imide lithium, wherein the yield of the crude bis (fluorosulfonyl) imide lithium is 95%;
2) Slowly adding 38g of crude bis (fluorosulfonyl) imide lithium obtained in the step 1) into a mixed solvent of 45g of diethyl ether, 5g of acetonitrile and 45g of dichloroethane for dissolving, obtaining a bis (fluorosulfonyl) imide lithium solution at 40 ℃ after the crude bis (fluorosulfonyl) imide lithium is completely dissolved, and cooling the bis (fluorosulfonyl) imide lithium solution to 25 ℃ for filtering; the filtrate was put on a rotary evaporator at 30 ℃ until the weight of the residue became 67g; slowly adding 50g of dichloroethane into the residue for crystallization, and filtering after crystallization to obtain a filter cake; washing the filter cake 3 times by using dichloroethane, wherein the weight of the dichloroethane used for each washing is 50g; and transferring the washed filter cake to a rotary evaporator for drying, and drying at 40 ℃ for 8h to obtain 30g of the lithium bis (fluorosulfonyl) imide. The yield of lithium bis (fluorosulfonyl) imide was 78.9% compared to the weight of crude lithium bis (fluorosulfonyl) imide.
Measuring the content of impurities in the obtained lithium bis (fluorosulfonyl) imide, wherein H 2 O：5ppm；K：1.5ppm；Na：1.2ppm；Fe<1ppm；Cl<1ppm；SO 4 2 ：3ppm。
Example 4
The embodiment provides a method for preparing lithium bis (fluorosulfonyl) imide, which comprises the following steps:
1) Adding 38.7g of bis (fluorosulfonyl) imide and 9.9g of lithium chloride into a reaction bottle, opening a gas absorption device, heating to enable materials in the reaction bottle to react for 5 hours at 130 ℃, blowing the materials in the reaction bottle by using nitrogen gas in the reaction process to remove hydrogen chloride gas generated by the reaction to obtain 36g of crude bis (fluorosulfonyl) imide lithium, wherein the yield of the crude bis (fluorosulfonyl) imide lithium is 90%;
2) Slowly adding 36g of crude bis (fluorosulfonyl) imide lithium obtained in the step 1) into a mixed solvent of 45g of diethyl ether and 45g of dichloroethane for dissolving, obtaining a bis (fluorosulfonyl) imide lithium solution after the crude bis (fluorosulfonyl) imide lithium is completely dissolved at 40 ℃, and cooling the bis (fluorosulfonyl) imide lithium solution to 25 ℃ for filtering; the filtrate was concentrated by vacuum evaporation in a rotary evaporator at 30 ℃ until the weight of the residue became 65g; slowly adding 50g of dichloroethane into the residue for crystallization, and filtering after crystallization to obtain a filter cake; washing the filter cake 3 times with dichloroethane, wherein the weight of the dichloroethane used in each washing is 50g; the washed filter cake was transferred to a rotary evaporator for drying and dried at 40 ℃ for 8 hours to obtain 32g of the lithium bis (fluorosulfonyl) imide. The yield of lithium bis (fluorosulfonyl) imide was 88.8% compared to the weight of crude lithium bis (fluorosulfonyl) imide.
Measuring the content of impurities in the obtained lithium bis (fluorosulfonyl) imide, wherein H 2 O：13ppm；K：16ppm；Na：15ppm；Fe<1ppm；Cl<1ppm；SO 4 2 ：9ppm。
Example 5
The embodiment provides a method for preparing lithium bis (fluorosulfonyl) imide, which comprises the following steps:
1) Adding 38.7g of bis (fluorosulfonyl) imide and 9.9g of lithium chloride into a reaction bottle, opening a gas absorption device, heating to enable materials in the reaction bottle to react for 5 hours at 130 ℃, blowing the materials in the reaction bottle by using nitrogen in the reaction process to remove hydrogen chloride gas generated by the reaction to obtain 36g of crude bis (fluorosulfonyl) imide lithium, wherein the recovery rate of the crude bis (fluorosulfonyl) imide lithium is 90%;
2) Slowly adding 36g of crude bis (fluorosulfonyl) imide lithium obtained in the step 1) into a mixed solvent of 45g of diethyl ether and 45g of toluene for dissolving, obtaining a bis (fluorosulfonyl) imide lithium solution after the crude bis (fluorosulfonyl) imide lithium is completely dissolved at 40 ℃, and cooling the bis (fluorosulfonyl) imide lithium solution to 25 ℃ for filtering; the filtrate was concentrated by vacuum evaporation in a rotary evaporator at 30 ℃ to a residue weight of 63g; slowly adding 50g of toluene into the residue for crystallization, and filtering after crystallization to obtain a filter cake; washing the filter cake 3 times by using toluene, wherein the weight of the toluene used for each washing is 50g; the washed filter cake was transferred to a rotary evaporator to be dried and dried at 40 ℃ for 8 hours to obtain 31g of the lithium bis (fluorosulfonyl) imide. The yield of lithium bis (fluorosulfonyl) imide was 86.1% compared to the weight of crude lithium bis (fluorosulfonyl) imide.
Measuring the content of impurities in the obtained lithium bis (fluorosulfonyl) imide, wherein H 2 O：5ppm；K：12ppm；Na：9ppm；Fe<1ppm；Cl<1ppm；SO 4 2 ：5ppm。
Example 6
1) Adding 38.7g of bis (fluorosulfonyl) imide and 9.9g of lithium chloride into a reaction bottle, opening a gas absorption device, heating to enable materials in the reaction bottle to react for 5 hours at 130 ℃, blowing the materials in the reaction bottle by using nitrogen gas in the reaction process to remove hydrogen chloride gas generated by the reaction to obtain 36g of crude bis (fluorosulfonyl) imide lithium, wherein the yield of the crude bis (fluorosulfonyl) imide lithium is 90%;
2) Slowly adding 36g of crude product of the lithium bis (fluorosulfonyl) imide obtained in the step 1) into a mixed solvent of 45g of diethyl ether, 5g of acetonitrile and 45g of dichloroethane for dissolving, obtaining a lithium bis (fluorosulfonyl) imide solution after the crude product of the lithium bis (fluorosulfonyl) imide is completely dissolved at 40 ℃, and cooling the lithium bis (fluorosulfonyl) imide solution to 25 ℃ for filtering; the filtrate was concentrated by vacuum evaporation in a rotary evaporator at 30 ℃ to a residual weight of 67g; slowly adding 50g of dichloroethane into the residue for crystallization, and filtering after crystallization to obtain a filter cake; washing the filter cake 3 times with dichloroethane, wherein the weight of the dichloroethane used in each washing is 50g; the washed filter cake was transferred to a rotary evaporator to be dried and dried at 40 ℃ for 8 hours to obtain 29g of the lithium bis (fluorosulfonyl) imide. The yield of lithium bis (fluorosulfonyl) imide was 80.5% compared to the weight of the crude lithium bis (fluorosulfonyl) imide.
Measuring the content of impurities in the obtained lithium bis (fluorosulfonyl) imide, wherein H 2 O：7ppm；K：7ppm；Na：5ppm；Fe<1ppm；Cl<1ppm；SO 4 2 ：3ppm。
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A preparation method of lithium bis (fluorosulfonyl) imide is characterized by comprising the following steps:
mixing the bis-fluorosulfonyl imide and lithium halide, reacting above the melting point of the bis-fluorosulfonyl imide to obtain a crude product of the bis-fluorosulfonyl imide, and purifying the crude product of the bis-fluorosulfonyl imide to obtain the lithium bis-fluorosulfonyl imide.
2. The method for preparing lithium bis (fluorosulfonyl) imide according to claim 1, wherein said reaction temperature is 124-150 ℃.
3. The method for producing lithium bis (fluorosulfonyl) imide according to claim 1 or 2, wherein,
the molar ratio of the bis-fluorosulfonyl imide to the lithium halide is (0.1-10): 1;
the reaction time is 5-24h;
the lithium halide is selected from at least one of lithium bromide, lithium iodide, lithium fluoride and lithium chloride, and preferably, the lithium halide is selected from at least one of lithium fluoride and lithium chloride.
4. The method for producing lithium bis (fluorosulfonyl) imide according to any one of claims 1 to 3, wherein no solvent is added during said reaction.
5. The method for preparing lithium bis (fluorosulfonyl) imide according to any one of claims 1 to 4, wherein said purification step comprises dissolving a crude lithium bis (fluorosulfonyl) imide to obtain a lithium bis (fluorosulfonyl) imide solution; and filtering, concentrating, crystallizing, filtering again, washing and drying the lithium bis (fluorosulfonyl) imide solution to obtain the lithium bis (fluorosulfonyl) imide.
6. The method for preparing lithium bis (fluorosulfonyl) imide according to claim 5, wherein the solvent for dissolving the crude lithium bis (fluorosulfonyl) imide comprises a first solvent and a second solvent, wherein the first solvent is at least one selected from the group consisting of diethyl ether, propyl ether, tetrahydrofuran, acetonitrile, ethyl acetate, propyl acetate, methyl acetate, dimethyl carbonate, diethyl carbonate, dioxane, acetone, and methyl ethyl ketone;
the second solvent is at least one selected from xylene, toluene, benzene, dichlorobenzene, chlorobenzene, difluorobenzene, fluorobenzene, petroleum ether, dichloromethane, dichloroethane, hexane and cyclohexane;
preferably, the first solvent is selected from at least one of diethyl ether, acetonitrile, dimethyl carbonate and diethyl carbonate; the second solvent is at least one selected from the group consisting of dichloromethane, dichloroethane, and toluene.
7. The method for producing lithium bis (fluorosulfonyl) imide according to claim 6,
the dissolving temperature is 0-100 ℃, and preferably, the dissolving temperature is 30-60 ℃;
the mass ratio of the crude product of the bis-fluorosulfonyl imide lithium to a solvent for dissolving the crude product of the bis-fluorosulfonyl imide lithium is 1: (1-3).
8. The method for producing lithium bis (fluorosulfonyl) imide according to any one of claims 5 to 7, wherein the crystallization solvent used in the crystallization step is at least one selected from the group consisting of xylene, toluene, benzene, dichlorobenzene, chlorobenzene, difluorobenzene, fluorobenzene, petroleum ether, dichloromethane, dichloroethane, hexane and cyclohexane;
the washing solvent used in the washing step is at least one selected from the group consisting of xylene, toluene, benzene, dichlorobenzene, chlorobenzene, difluorobenzene, fluorobenzene, petroleum ether, dichloromethane, dichloroethane, hexane and cyclohexane.
9. The method for producing lithium bis (fluorosulfonyl) imide according to any one of claims 5 to 8, wherein said drying temperature is 40 to 80 ℃; the drying time is 3-10h.
10. Use of the lithium bis (fluorosulfonyl) imide prepared by the method of any one of claims 1 to 9 in the preparation of an electrolyte material for lithium ion batteries.
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| CN117175015A (en) * | 2023-11-02 | 2023-12-05 | 深圳新宙邦科技股份有限公司 | Nonaqueous electrolyte and battery |
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| CN106365132A (en) * | 2016-08-31 | 2017-02-01 | 中国船舶重工集团公司第七八研究所 | Preparation method of difluoro-sulfimide and lithium difluoro-sulfimide |
| CN113511639A (en) * | 2021-06-17 | 2021-10-19 | 深圳市研一新材料有限责任公司 | Lithium bis (fluorosulfonyl) imide and preparation method and application thereof |
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| CN115959636A (en) * | 2022-12-21 | 2023-04-14 | 浙江研一新能源科技有限公司 | Preparation method of lithium bis (fluorosulfonyl) imide and lithium ion battery |
| CN117175015A (en) * | 2023-11-02 | 2023-12-05 | 深圳新宙邦科技股份有限公司 | Nonaqueous electrolyte and battery |
| CN117175015B (en) * | 2023-11-02 | 2024-04-05 | 深圳新宙邦科技股份有限公司 | Nonaqueous electrolyte and battery |
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